反应详情

A mixture of 246 mg (1 mmol) (5-hydroxy-1H-indol-2-yl)-morpholin-4-yl-methanone, 1 g (ca. 3 mmol) polymerbound triphenylphospine (Fluka), 179 mg (1.25 mmol) piperidinepropanol and 461 mg (2 mmol) di-tert.-butyl azadicarboxylate in 20 ml THF was stirred for a prolonged period of time at room temperature. The mixture was filtered through a pad of silica and washed with 30 ml THF. The mixture was evaporated to dryness and purified on silica eluting with a gradient of DCM/2N NH3 in methanol 98/2 to DCM/2N NH3 in methanol 9/1. The product fractions were evaporated and the residue was titurated with diethyl ether to yield after drying at 40° C. under vacuum 47 mg (13%) of the title compound as white solid. MS (m/e): 372.4 (MH+, 100%).

1. filtrationThe mixture was filtered through a pad of silica
2. washwashed with 30 ml THF
3. customThe mixture was evaporated to dryness
4. custompurified on silica eluting with a gradient of DCM/2N NH3 in methanol 98/2 to DCM/2N NH3 in methanol 9/1
5. customThe product fractions were evaporated
6. customto yield
7. dry with materialafter drying at 40° C. under vacuum 47 mg (13%) of the title compound as white solid